UHPLC/ESI Q-Orbitrap Quantitation of 655 Pesticide Residues in Fruits and Vegetables—A Companion to an nDATA Working Flow

2020 ◽  
Vol 103 (6) ◽  
pp. 1547-1559
Author(s):  
Jian Wang ◽  
Daniel Leung ◽  
Willis Chow ◽  
Jon W Wong ◽  
James Chang
Keyword(s):  
Pesticide Residues ◽  
High Performance ◽  
Fruits And Vegetables ◽  
Residue Analysis ◽  
Resolving Power ◽  
Intermediate Precision ◽  
Monitoring Programs ◽  
Routine Monitoring ◽  
Mass Resolving Power ◽  
Chromatographic Resolution

Abstract Background Effective and expansive methods for multiresidue pesticide analysis are desired for routine monitoring programs. These methods are complex, especially when several hundred pesticides are involved. Objective Two approaches to sort data and identify isomers and isobaric ions in pesticide mixtures were evaluated to determine whether they could be differentiated by mass resolving power and/or chromatographic resolution. Method This study presents an application of ultra-high performance liquid chromatography electrospray Q-Orbitrap mass spectrometry (UHPLC/ESI Q-Orbitrap) along with QuEChERS for the quantitation of 655 pesticide residues in fruits and vegetables. Results From the developed method, 94.7% of the 655 pesticides in fruits and 93.9% of those in vegetables had recoveries between 81% and 110%; 98.3% in both fruits and vegetables had an intermediate precision of ≤20%; and 97.7% in fruits or 97.4% in vegetables showed measurement uncertainty of ≤50%. When the retention time difference (ΔtR) of two isomers was ≥0.12 min, they were chromatographically resolved. Twenty five out of 35 pairs or groups of isomers were chromatographically separated (ΔtR ≥ 0.12 min), but 14 pairs were not resolved (ΔtR < 0.12 min). There were 493 pairs of pesticides with a mass-to-charge difference of <1 Da. Only one pair of isobaric ions could not be separated by mass and chromatographic resolution. Highlights UHPLC/ESI Q-Orbitrap along with QuEChERS sample preparation offers a practical quantitative companion method to a non-target data acquisition for target analysis workflow for pesticide residue analysis in routine monitoring programs for food safety.

A Complementary, Quantitative and Confirmatory Method to UHPLC/ESI Q-Orbitrap Screening based on UPHLC/ESI-MS/MS for Analysis of 416 Pesticides in Fruits and Vegetables

2021 ◽  
Author(s):  
Willis Chow ◽  
Daniel Leung ◽  
Jian Wang
Keyword(s):  
Pesticide Residues ◽  
High Performance ◽  
Fruits And Vegetables ◽  
Method Development ◽  
Multiple Reaction Monitoring ◽  
Extraction Procedure ◽  
Screening Methods ◽  
Intermediate Precision ◽  
Esi Ms ◽  
Measurement Uncertainties

Abstract Background Triple quadrupole (MS/MS) and high-resolution mass spectrometer (HRMS), coupled with ultra-high performance liquid chromatography (UHPLC) or gas chromatography (GC), are technologies used to analyse pesticide residues in fruits and vegetables. LC-MS/MS has been the gold standard for analysis of pesticides, offering reliable performance and sensitivity, while LC-HRMS is expanding in applications to serve as another benchmark. Method development and testing scope expansion are constantly required with new generation mass spectrometers. Objective This paper discusses the development and validation of a quantitative and confirmatory method that can analyse over 400 pesticide residues using state-of-the-art UHPLC/ESI-MS/MS system. Method Homogenized fruit and vegetable samples were fortified with pesticides and were extracted using a modified QuEChERS method. Samples were injected onto a UHPLC/ESI-MS/MS system, and data were acquired in multiple reaction monitoring mode. The method was validated using a nested experimental design, and was able to quantify and confirm 416 pesticide in fruits and vegetables. It was also complimentary to the UHPLC/ESI Q-Orbitrap quantitative and screening methods previously developed in the authors’ laboratory. Results The method demonstrated good performance. In all matrices, 92% of pesticides yielded recoveries between 81–110%, more than 95% of pesticides yielded intermediate precision ≤ 20%, and about 65% of pesticides yielded measurement uncertainties ≤ 20%, and 96% of pesticides yielded measurement uncertainties ≤ 50%. Highlights This method was developed using the same mobile phases, analytical columns, and extraction procedure, as UHPLC/ESI Q-Orbitrap methods. Extracts can be run on either system, streamlining monitoring programs and offering high sample throughput.

Evaluation of an alternative fluorinated chitosan as a QuEChERS adsorbent for pesticide residue analysis in apple samples

2019 ◽  
Vol 11 (27) ◽  
pp. 3460-3466 ◽  
Author(s):  
Qilin Deng ◽  
Liping Sun ◽  
Tao Zhu
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Pesticide Residue ◽  
Pesticide Residues ◽  
High Performance ◽  
Residue Analysis ◽  
Pesticide Residue Analysis ◽  
Quechers Method

In this study, a new and green fluorinated chitosan (trifluoroethyl methacrylate-chitosan (TFEMA-CTS)) was synthesized, and the QuEChERS method was applied for the effective determination of four pesticide residues in apple samples by high performance liquid chromatography.

scholarly journals Quantitative analysis of fresh tomatoes (Solanum lycopersicum) for trace of pesticide residues from markets in Peshawar, Pakistan, using High Performance Thin Liquid Chromatography technique

2020 ◽  
Vol 23 (3) ◽  
pp. 708-714
Author(s):  
Syeda Kokab Shah ◽  
Syeda Faryal Israr ◽  
Asif Khan Khatak ◽  
Abeer Kazmi ◽  
Amir Ali ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Solanum Lycopersicum ◽  
Pesticide Residues ◽  
High Performance ◽  
Fruits And Vegetables ◽  
Phase 1 ◽  
Research Work ◽  
Efficient Approach ◽  
Maximum Residue Levels ◽  
Residue Levels

Background: Vegetables and fruits are vital constituents of human diet, as it provides necessary minerals and nutrients to human body to carry out biological reactions and provide protection against various diseases and injuries. Solanum lycopersicum (tomato) is consider as cash crop in Asian countries and are fine source of vitamin C, potassium, folate, vitamin K, and other bioactive compounds including, phenolics, flavonoids, carotenoids, and alkaloids. Similar to other crops, tomato quality and yield is also affected by pests. Globally, approximately 37.8% of tomato yield is spoiled due to pests. To maintain the vegetable quality and attain more yield, pest management approaches are applied, though extensive use of toxic pesticides are becoming a part of our food chain and causing adverse effects. Methodology: The present research is intended to evaluate the levels of toxic pesticides in different tomato varieties collected from four vegetable markets (Hayatabad Phase 1, Chargano Chowk, Kohat Road and Tarnab farm) in Peshawar, Pakistan. After collection of tomato samples, level of pesticide residues (Cyhalothrin, Cypermethrin, Chlorpyrifos, Bifenthrin, and Imidacloprid) were detected using high performance thin liquid Chromatography (HPTLC). Results: After detection, level of pesticides in sample was compared with Maximum residue levels (MRLs). The magnitude of pesticides in samples was lesser to the Maximum residue levels (MRLs) provided by United State Drug Agency (USDA), though the quantity of Lambda Cyhalothrin present in the sample was almost equal to MRL (0.097 mg/kg). Conclusion: HPTLC is an efficient approach to detect pesticide traces in fruits and vegetables. Research work should be focused on it, to identify and control farmer practices which are highly linked to pesticide contamination in tomatoes and use of biopesticides should be encouraged. The cultivation of transgenic tomatoes can also be an efficient approach to elude the utilization of toxic pesticides.

scholarly journals Evaluation of Some Pesticide Residues in Fruits import by High Performance Liquid Chromatography

2017 ◽  
Vol 27 (4) ◽  
Author(s):  
Lamees M. A. Salman ◽  
Iyad Abdul-Muhsan Ahmed
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Pesticide Residues ◽  
High Performance ◽  
Fruits And Vegetables ◽  
Current Knowledge ◽  
Maximum Residue Limits ◽  
Exposure Risks ◽  
Core Mixture

Pesticide residues have been found in various fruits and vegetables.  This study collected 24 samples and reported a method based on High Performance Liquid Chromatography (HPLC). For determination of pesticide residues used in Some fruits which were collected from different markets of Baghdad city to make) 24)  samples from (peel , core, mixture) for each type of fruits markets as:  Oranges( Egypt , Africa), Pomegranate ( Egypt), Mango ( Kenya ), Pears (China),  Plum fruits ( Africa ) , Kiwi (Turkey ) .That detective of ( 5 ) different  pesticides (diazinon,  malathion, chlorpyrifos ,parathion  and cypermethrin). The results were detected of multi-residues of  pesticides on the fruit in ( peel , core , mixture ) may be in the limit of Maximum residue limits(MRL) or higher of it   . The pesticides detected that exceeding the limits are: cypermethrin  in Kiwi (peel, core and mixture)at(0.204,0.038, 0.537), in pomegranate detected in (peel and mixture) at (0.509,0.189) mg/kg , Diazinon detccted in Egyptian orange in (peel ,core and mixture) at (0.031,0.207, 0.099) mg/kg . Malathion and Parathion was not detected at any type of fruits and  that results was compared with codex of FAO/WHO(2013). That data is important to monitor residues in food and to fill gaps in current knowledge would be helpful in assessing human exposure risks from ingestion of contaminated Fruits Imported to our country.

scholarly journals Fate of Preharvest-Sprayed Dicofol in Date Fruits: Residue Analysis by HPLC-UV

2005 ◽  
Vol 10 (1) ◽  
pp. 21 ◽  
Author(s):  
S. Al-Rehiayani ◽  
K.A. Osman
Keyword(s):  
High Performance ◽  
Fruits And Vegetables ◽  
Date Palm ◽  
Residue Analysis ◽  
Second Phase ◽  
Time Intervals ◽  
Biphasic Model ◽  
Palm Trees ◽  
Recovery Percentage ◽  
Date Fruits

The fate of pre-harvest-sprayed dicofol (DCF) on date fruits has been investigated. Date palm trees, variety Sukkari, were sprayed with DCF (18.5%, EC) at the rate of 200 ml/100 L. DCF residues in date fruits were determined at different time intervals using high performance liquid chromatography (HPLC) with UV detection at 220 nm. The method was based on extraction with ethyl acetate. The results showed that the HPLC response was linear (r2 > 0.98) for DCF in the range of 0.0 to 2 mμg. The limits of detection and quantification were 0.24 and 0.80 ppm, respectively. The method was developed by using spiked date fruits at levels of 0.25, 0.50 and 1.0 ppm. Recovery percentage was satisfactory with a range of 77.2 to 103.6% and an RSD ranging from 6.33 to 11.84%. A biphasic model was assumed in order to carry out the statistical study of the loss of DCF from date fruits. The results showed that the initial deposit of DCF on date fruits was 11.22 ppm, while the residue value decreased to 1.90 ppm seven days after spraying, which is below the tolerance limit for fruits and vegetables (2 ppm). Also, the data indicate that there was a faster rate of DCF loss in the first phase than the second one. This is clearly reflected in the t1/2 values, where the half-lives of DCF were 1.35 and 38.52 days, for the first and second phase model, respectively. The described method is rapid and sensitive, with satisfactory recoveries and reproducibility. 

Pesticide Residues in Milk and Fish Samples Collected from Two Egyptian Governorates

1990 ◽  
Vol 73 (1) ◽  
pp. 19-21 ◽  
Author(s):  
Salwa M Dogheim ◽  
Eslam N Nasr ◽  
Monir M Almaz ◽  
Mahmoud M EL-Tohamy
Keyword(s):  
Pesticide Residues ◽  
Residue Analysis ◽  
Monitoring Program ◽  
Milk Samples ◽  
Monitoring Programs ◽  
Future Needs ◽  
Fish Samples ◽  
Intensive Use ◽  
Fayoum Governorate ◽  
Do So

Abstract Because of the intensive use of pesticides for the control of certain pests In Egypt, country-wide residue monitoring programs must be established that can cover all the Egyptian Governorates exposed to pesticide treatments. To do so, limited programs must be adopted first, so that current situations and future needs for improved programs are identified. The present paper reports results from a limited monitoring program, which started in 1985 in one governorate and then expanded to include another in 1986. Fish and milk samples were the commodities selected for residue analysis. The results showed that milk samples collected from Beni-Suef Governorate in 1986 had lower levels of organochlorine residues compared to those collected in 1985. Residues in boltifish and catfish samples in 1986 were much higher than those detected in 1985. In comparison with Beni-Suef Governorate, and contrary to expectations, milk derived from Fayoum Governorate in 1986 was more contaminated with pesticides. While the amount of residues in boltifish was comparatively higher, catfish samples were less contaminated.

Multi-residue analysis of pesticide residues in fruits and vegetables using gas and liquid chromatography with mass spectrometric detection

2018 ◽  
Vol 23 (3) ◽  
pp. 145-175 ◽  
Author(s):  
Despo Louca Christodoulou ◽  
Olympiada Kourouzidou ◽  
Militsa Hadjigeorgiou ◽  
Panayiota Hadjiloizou ◽  
Maria Constantinou ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Pesticide Residues ◽  
Fruits And Vegetables ◽  
Residue Analysis ◽  
Mass Spectrometric ◽  
Mass Spectrometric Detection ◽  
Gas And Liquid Chromatography
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